CN115924951B - Preparation method of calcium fluoride powder for cores - Google Patents
Preparation method of calcium fluoride powder for cores Download PDFInfo
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- CN115924951B CN115924951B CN202211649633.6A CN202211649633A CN115924951B CN 115924951 B CN115924951 B CN 115924951B CN 202211649633 A CN202211649633 A CN 202211649633A CN 115924951 B CN115924951 B CN 115924951B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 92
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 title claims abstract description 40
- 229910001634 calcium fluoride Inorganic materials 0.000 title claims abstract description 40
- 239000000843 powder Substances 0.000 title claims abstract description 23
- 239000007788 liquid Substances 0.000 claims abstract description 65
- 230000000694 effects Effects 0.000 claims abstract description 46
- 238000001914 filtration Methods 0.000 claims abstract description 44
- 238000001179 sorption measurement Methods 0.000 claims abstract description 43
- 238000007599 discharging Methods 0.000 claims abstract description 12
- 238000002347 injection Methods 0.000 claims abstract description 9
- 239000007924 injection Substances 0.000 claims abstract description 9
- 238000000926 separation method Methods 0.000 claims abstract description 9
- 238000009833 condensation Methods 0.000 claims abstract description 6
- 230000005494 condensation Effects 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 78
- 238000001514 detection method Methods 0.000 claims description 54
- 238000006243 chemical reaction Methods 0.000 claims description 35
- 230000009471 action Effects 0.000 claims description 28
- 238000003756 stirring Methods 0.000 claims description 27
- 230000005540 biological transmission Effects 0.000 claims description 25
- 230000018044 dehydration Effects 0.000 claims description 24
- 238000006297 dehydration reaction Methods 0.000 claims description 24
- 238000005406 washing Methods 0.000 claims description 22
- 239000012153 distilled water Substances 0.000 claims description 21
- 239000011148 porous material Substances 0.000 claims description 21
- 239000002994 raw material Substances 0.000 claims description 21
- 239000004744 fabric Substances 0.000 claims description 20
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 16
- 239000007787 solid Substances 0.000 claims description 15
- MIMUSZHMZBJBPO-UHFFFAOYSA-N 6-methoxy-8-nitroquinoline Chemical compound N1=CC=CC2=CC(OC)=CC([N+]([O-])=O)=C21 MIMUSZHMZBJBPO-UHFFFAOYSA-N 0.000 claims description 11
- 239000002351 wastewater Substances 0.000 claims description 11
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 8
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 6
- 229910052731 fluorine Inorganic materials 0.000 claims description 6
- 239000011737 fluorine Substances 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 230000010355 oscillation Effects 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 4
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 239000003507 refrigerant Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims description 2
- 239000000243 solution Substances 0.000 abstract description 6
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 230000000903 blocking effect Effects 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 229910052770 Uranium Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- DNYWZCXLKNTFFI-UHFFFAOYSA-N uranium Chemical compound [U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U] DNYWZCXLKNTFFI-UHFFFAOYSA-N 0.000 description 2
- 101100314150 Caenorhabditis elegans tank-1 gene Proteins 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- MZFRHHGRNOIMLW-UHFFFAOYSA-J uranium(4+);tetrafluoride Chemical compound F[U](F)(F)F MZFRHHGRNOIMLW-UHFFFAOYSA-J 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
Landscapes
- Removal Of Specific Substances (AREA)
- Separation Of Gases By Adsorption (AREA)
Abstract
The invention discloses a preparation method of calcium fluoride powder for a core, which relates to the field of calcium fluoride, and comprises a preparation tank, wherein a discharging bin playing a role in quantitative discharging and a liquid injection port playing a role in liquid injection are fixedly arranged at the top of the preparation tank, a preparation assembly is arranged at the left end of the preparation tank, a multidirectional flow guiding effect is provided for preparing a solution through a guiding pump and a first reversing valve, intelligent control is performed on each preparation step through a second reversing valve and other parts, the intelligent control effect on the preparation steps is improved, a gas filtering assembly is arranged at the left end of the preparation tank, gas in the liquid is separated through the condensation effect of an adsorption inner cylinder and a heat exchange tube, and the gas-liquid separation effect is improved through the swirling effect of a baffle plate.
Description
Technical Field
The invention relates to the field of calcium fluoride, in particular to a preparation method of calcium fluoride powder for cores.
Background
Calcium fluoride is an inorganic compound, has a chemical formula of CaF2 and is colorless crystal or white powder; hardly soluble in water and slightly soluble in inorganic acid, and reacts with hot concentrated sulfuric acid to generate hydrofluoric acid; in the process of preparing metal uranium in nuclear industry, a method of reducing uranium tetrafluoride by calcium is generally adopted, and in order to avoid the metal container being melted at high temperature to lead impurities to be introduced into the metal uranium, a substance calcium fluoride which is the same as a reaction byproduct is lined between a reaction material and the reaction metal container; many materials are used as refractory lining, such as calcium fluoride, graphite, magnesium oxide, calcium oxide, etc., with high purity calcium fluoride being the most desirable refractory lining.
In the prior art, a plurality of preparation raw materials are mostly directly added in proportion in the preparation process, the priority of the sequential reaction procedures of the plurality of raw materials is not ordered, and a detection part for carrying out acid-base data on the mixed liquid in the preparation process is also not needed;
Meanwhile, more equipment is needed in the preparation process in the prior art, so that the whole device in the prior art is large in size, a large amount of manpower is needed for auxiliary addition and operation in the preparation process, the degree of automation is poor, and the labor cost in the preparation process in the prior art is high.
Disclosure of Invention
Accordingly, in order to solve the above-mentioned disadvantages, the present invention provides a method for producing a calcium fluoride powder for nuclear use.
The invention is realized in such a way, and a preparation method of calcium fluoride powder for nuclear is constructed, the device comprises a preparation tank, wherein the top of the preparation tank is fixedly provided with a discharging bin with a quantitative discharging function and a liquid injection port with a liquid injection function;
The preparation assembly is arranged at the left end of the preparation tank and comprises a guiding-out pump, and the bottom through holes of the preparation tank and the reaction tank are connected with a water inlet pipeline at the top of the guiding-out pump through connecting pipes; the water outlet pipeline at the rear end of the guide pump is provided with a first reversing valve which plays a role in guiding; the left end of the first reversing valve is fixedly provided with the air filtering component through a connecting pipe; the bottom pipeline of the air filtering component is provided with a second reversing valve which plays a role in control; the bottom of the second reversing valve is provided with a dehydration assembly which plays a role in dehydration; the water inlet pipeline at the rear end of the second reversing valve is provided with a first external connecting pipe; the water outlet pipeline at the rear end of the first reversing valve is provided with a reflux pipe which plays a reflux role; the rear end of the return pipe is provided with a detection component which plays a role in detection; the top of the detection component is provided with a second outer connecting pipe; the connection parts at the outer sides of the first outer connecting pipe and the second outer connecting pipe are respectively provided with a quick connector, and the leading-out pump, the first reversing valve and the second reversing valve are electrically connected with the controller.
Preferably, the air filtering component comprises a temperature control outer cylinder, and the top side of the left end of the preparation tank is fixedly provided with the temperature control outer cylinder; an adsorption inner cylinder which plays a role in separation and adsorption is fixedly arranged on the inner side wall of the temperature control outer cylinder through bolts; the heat exchange tube is adhered and fixed on the outer side wall of the adsorption inner cylinder and has a heat exchange effect; the water inlets and the water outlets on the upper side and the lower side of the heat exchange tube are connected with an external valve pipeline; the baffle plate is fixedly welded on the inner side wall of the adsorption inner cylinder and plays a role in stirring flow; the air guiding pipe is welded and fixed at the central through hole of the baffle plate; the quick connector is arranged on the pipeline at the top of the air outlet pipe; wherein, the absorption inner tube inside wall is equipped with the slot that plays the choked flow effect.
Preferably, the dehydration component comprises a dehydration cylinder, and a water cylinder which plays a dehydration role is fixedly arranged at the bottom side of the left end of the preparation tank; the water outlet pipeline at the bottom of the dehydration cylinder is provided with a third reversing valve, and the bottom of the third reversing valve is arranged with the bottom pipeline of the first reversing valve through a connecting pipe; the bottom of the inner part of the dewatering cylinder is rotatably provided with a fine pore filter cylinder which plays a role in filtering through a bracket; the inner side wall of the fine pore filter cylinder is adhered and fixed with water filtering cloth which plays a role in filtering; the toothed ring is arranged on the outer side of the connecting plate at the top of the fine-pore filter cylinder through bolts, and the toothed ring has a transmission function; the outer side of the toothed ring is meshed with the rear end of the transmission gear; the center hole of the transmission gear is connected with a transmission shaft key of the servo motor; the servo motor bolt is arranged in the protective box at the front side of the dewatering cylinder, and the third reversing valve and the servo motor are electrically connected with the controller.
Preferably, the detection assembly comprises a connecting sleeve, and the rear end pipeline of the return pipe is provided with the connecting sleeve which plays a role in guiding flow; the rear end pipeline of the connecting sleeve is provided with a fourth reversing valve which plays a role in guiding; the fourth reversing valve pipeline is arranged at the bottom of the detection cylinder; the fifth reversing valve is arranged on the pipeline at the top of the detection cylinder and plays a role in guiding; the left end bolt of the detection cylinder is provided with a magnet vibrator which plays a role in detection; the detector is mounted at the rear end bolt of the detection cylinder; the upper side of the front end of the detector is fixedly provided with a sample measuring electrode through a lead; the reference electrode is fixedly arranged on the lower side of the front end of the detector through a wire; the fourth reversing valve, the fifth reversing valve, the magnet vibrator, the detector, the sample measuring electrode and the reference electrode are all electrically connected with the controller.
Preferably, the middle side bolt at the top of the preparation tank is provided with a transmission motor and a controller arranged at the front side of the preparation tank by bolts, a stirring paddle playing a role in stirring is fixedly arranged at a transmission shaft at the bottom of the transmission motor, the stirring paddle is rotationally arranged inside the reaction tank, and a hot water guide pipe is arranged at the bottom side of the front end of the preparation tank.
Preferably, the baffle is spirally distributed at the inner wall of the adsorption inner cylinder, and the diameter of the central through hole of the baffle and the diameter of the air guiding-out pipe.
Preferably, the filter screen diameters of the fine-pore filter cartridge and the water filtering cloth are 1 cm and 1 mm respectively.
Preferably, the front end of the dehydration cylinder is provided with a connecting box body which plays a role in protecting the servo motor.
Preferably, the top of the fourth reversing valve and the bottom of the fifth reversing valve are respectively provided with a second external connecting pipe, and quick connectors are respectively arranged at the ends of the two groups of second external connecting pipes.
Preferably, the preparation method of the calcium fluoride powder for the core comprises the following preparation steps:
Quantitatively adding distilled water and ammonium bifluoride raw materials: adding quantitative distilled water into a reaction tank in a preparation tank, introducing external hot water into the preparation tank through a hot water conduit, heating the distilled water in the reaction tank, controlling the temperature of the external hot water to enable the distilled water to be kept at 60-80 ℃, adding quantitative ammonium bifluoride raw material into the reaction tank, proportioning the ammonium bifluoride raw material and distilled water at a solid-to-liquid ratio of 1:5, and controlling a transmission motor to work through a controller and driving a stirring paddle to stir, so that the ammonium bifluoride raw material and distilled water are fully dissolved;
Step two: quantitative and slow addition of calcium carbonate raw material: then the calcium carbonate raw material is slowly and quantitatively introduced into the reaction tank through the vibration of the discharging bin and is dissolved through stirring, and the ratio of the calcium carbonate raw material to the mixed liquid is 1:7, keeping the temperature inside the reaction tank between 60 and 80 ℃ under the action of the heat of the hot water conduit, fully reacting under the stirring action of the stirring paddle, and guiding the mixed solution into the detection assembly for detection under the driving action of the guiding-out pump and the first reversing valve;
Step three: and (3) guiding out filtered gas: then, the mixed liquid in the reaction tank is guided out through the guiding-out pump and flows into the adsorption inner cylinder under the driving action of the first reversing valve, guiding-out pressure is provided for the liquid through the guiding-out pump at the moment, so that the mixed liquid with reaction crystals forms a rotational flow state under the flow blocking action of the baffle plate, and meanwhile, an external refrigerant is guided into the heat exchange tube through the external valve, so that the whole heat of the adsorption inner cylinder is taken away, the mixed liquid can be contacted with the inner wall of the adsorption inner cylinder under the action of rotational flow centrifugation, so that the gas in the mixed liquid can be contacted with the adsorption inner cylinder under the condensation action of the liquid to separate from the liquid, liquid particles can be attached to the inner side of the adsorption inner cylinder, and the gas generated by reaction in the mixed liquid is prevented from being taken away by the air flow through the groove strips on the inner side of the adsorption inner cylinder, and separation of the gas generated by reaction is facilitated;
step four: and (3) centrifugal dehydration: then introducing the deaerated mixed liquid into a dehydration assembly under the action of a second reversing valve, collecting the inflow mixed liquid through a fine-hole filter cylinder and a water filtering cloth, controlling a servo motor to drive a transmission gear to rotate and enable the transmission gear to be meshed with a toothed ring through a controller, enabling the toothed ring to drive the fine-hole filter cylinder and the water filtering cloth to rotate, separating redundant fluorine-containing wastewater from calcium fluoride solids through the filtering effect of the fine-hole filter cylinder and the water filtering cloth and centrifugal force during rotation, and guiding the redundant fluorine-containing wastewater out through a third reversing valve;
step five: repeat the washing: external distilled water is led into the fine pore filter cylinder through the flow guiding effect of the second reversing valve and the second outer connecting pipe to flush and wash calcium fluoride solids;
Step six: and (3) PH value detection: at the moment, the washing wastewater is led into the first reversing valve due to the reversing effect of the third reversing valve, flows into the detection cylinder through the reversing effects of the first reversing valve and the fourth reversing valve, and is controlled by the controller to perform oscillation work by the magnetite vibrator, the sample measuring electrode and the reference electrode are subjected to oscillation waves to generate detection data and are transmitted to the detector, the detector monitors the washing PH value through two groups of data, and the PH value of liquid and solid is kept consistent in the washing process, so that PH value data of calcium fluoride solid is also obtained;
Step seven: grinding and pulverizing: when the PH value data reaches the standard value, the repeated washing is stopped, and the calcium fluoride solid is taken out for drying and grinding.
The invention has the following advantages: the invention provides a preparation method of calcium fluoride powder for cores, which is improved compared with the same type of equipment by improvement, and has the following improvements:
according to the preparation method of the calcium fluoride powder for the core, the preparation assembly is arranged at the left end of the preparation tank, the guiding pump and the first reversing valve provide a multidirectional flow guiding effect for preparing the solution, and the intelligent control of all preparation steps is carried out through the second reversing valve and other parts, so that the intelligent control effect on the preparation steps is improved.
According to the preparation method of the calcium fluoride powder for the nuclear, the gas filtering component is arranged at the left end of the preparation tank, gas in liquid is separated through the condensation effect of the adsorption inner cylinder and the heat exchange tube, and the preparation solution is enabled to generate centrifugal force through the cyclone effect of the baffle plate, so that the gas-liquid separation effect is improved.
According to the preparation method of the calcium fluoride powder for the core, the dehydration component is arranged at the left end of the preparation tank, the fine pore filter cylinder and the toothed ring are driven by the servo motor to rotate at high speed, solids are blocked under the filtering action of the fine pore filter cylinder and the water filtering cloth, and the dehydration and washing effects on solid materials are improved.
According to the preparation method of the calcium fluoride powder for the nuclear, the detection assembly is arranged at the rear side of the preparation tank, the detection cylinder and the return pipe can form a return closed loop under the reversing and guiding actions of the third reversing valve and the fourth reversing valve, and the PH value of the preparation material is detected by the magnet vibrator and the detector under the multiple data detection actions of the sample detection electrode and the reference electrode.
Drawings
FIG. 1 is a schematic flow chart of the steps of the present invention;
FIG. 2 is a schematic perspective view of a manufacturing tank and manufacturing assembly of the present invention;
FIG. 3 is a schematic perspective cross-sectional structure of a preparation assembly of the present invention;
FIG. 4 is a schematic view of the internal structure of the air filter assembly of the present invention;
FIG. 5 is a schematic perspective view of the adsorption inner cylinder and heat exchange tube of the present invention;
FIG. 6 is a schematic perspective cross-sectional view of the dewatering assembly of the present invention;
FIG. 7 is a schematic perspective view of a detection assembly according to the present invention;
Fig. 8 is a schematic perspective exploded view of the detection assembly of the present invention.
Wherein: the preparation tank-1, the preparation assembly-2, the discharging bin-3, the liquid injection port-4, the transmission motor-5, the controller-6, the stirring paddle-7, the reaction tank-8, the hot water conduit-9, the leading-out pump-21, the first reversing valve-22, the gas filtering assembly-23, the second reversing valve-24, the dehydration assembly-25, the first outer connecting pipe-26, the return pipe-27, the detection assembly-28, the second outer connecting pipe-29, the temperature control outer cylinder-231, the adsorption inner cylinder-232, the heat exchange tube-233, the outer connecting valve-234, the baffle plate-235, the gas outlet tube-236, the quick connector-237, the dehydration cylinder-251, the third reversing valve-252, the pore filter cylinder-253, the water filtering cloth-254, the toothed ring-255, the transmission gear-256, the servo motor-257, the connecting sleeve-281, the fourth reversing valve-282, the detection cylinder-283, the fifth reversing valve-284, the magnetite vibrator-285, the detector-286, the sample measuring electrode-287, and the reference electrode-288.
Detailed Description
The principles and features of the present invention are described below with reference to fig. 1-8, the examples being provided for illustration only and not for limitation of the scope of the invention. The invention is more particularly described by way of example in the following paragraphs with reference to the drawings. Advantages and features of the invention will become more apparent from the following description and from the claims. It should be noted that the drawings are in a very simplified form and are all to a non-precise scale, merely for convenience and clarity in aiding in the description of embodiments of the invention.
It will be understood that when an element is referred to as being "fixed to" another element, it can be directly on the other element or intervening elements may also be present. When a component is considered to be "connected" to another component, it can be directly connected to the other component or intervening components may also be present. When an element is referred to as being "disposed on" another element, it can be directly on the other element or intervening elements may also be present. The terms "vertical," "horizontal," "left," "right," and the like are used herein for illustrative purposes only.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
Referring to fig. 1-8, the preparation method of calcium fluoride powder for nuclear use of the invention comprises a preparation tank 1, the preparation tank 1, a discharging bin 3 playing a role in quantitative discharging and a liquid injection port 4 playing a role in liquid injection are fixedly arranged at the top of the preparation tank 1, a transmission motor 5 and a controller 6 which is arranged at the front side of the preparation tank 1 are arranged on a bolt at the middle side of the top of the preparation tank 1, a stirring paddle 7 playing a role in stirring is fixedly arranged on a transmission shaft at the bottom of the transmission motor 5, the stirring paddle 7 is rotatably arranged in the reaction tank 8, and a hot water guide pipe 9 is arranged at the bottom side of the front end of the preparation tank 1.
Still including setting up the preparation subassembly 2 in preparation jar 1 left end, preparation subassembly 2 includes and derives pump 21, preparation jar 1 and retort 8 bottom through-hole all are connected with deriving pump 21 top water inlet pipeline through the connecting tube, derive pump 21 rear end delivery port pipeline installs the first switching-over valve 22 that plays the guide effect, it provides the switching-over effect to derive pump 21 direction of deriving through first switching-over valve 22, first switching-over valve 22 left end is through connecting tube fixed mounting has gas filtering subassembly 23, gas filtering subassembly 23 bottom pipeline installs the second switching-over valve 24 that plays the control effect, second switching-over valve 24 bottom is equipped with the dehydration subassembly 25 that plays the dehydration effect, first outer takeover 26 is installed to second switching-over valve 24 rear end water inlet pipeline, distilled water through the leading-in washing of first outer takeover 26, first switching-over valve 22 rear end delivery port pipeline installs the back flow 27 that plays the backward flow effect, the back end of back flow 27 is equipped with the detection component 28 that plays the detection effect, the detection component 28 top is equipped with second outer takeover 29, first outer takeover 26 and second outer 29 outside junction all is equipped with quick-operation, derive pump 21, first outer takeover valve 22 and second switching-over valve 24 and second switching-over valve 6 are all connected with electric energy for second switching-over valve 24, electric energy and second switching-over valve 6.
The air filtering assembly 23 comprises a temperature control outer cylinder 231, the top side of the left end of the preparation tank 1 is fixedly provided with the temperature control outer cylinder 231, the inner side wall of the temperature control outer cylinder 231 is fixedly provided with an adsorption inner cylinder 232 which plays a role in separation and adsorption through bolts, a concentrated converging effect is provided for mixed liquid through the adsorption inner cylinder 232, the outer side wall of the adsorption inner cylinder 232 is fixedly adhered with a heat exchange tube 233 which plays a role in heat exchange, water inlet and outlet ports on the upper side and the lower side of the heat exchange tube 233 are all connected with an external valve 234 through pipelines, the inner side wall of the adsorption inner cylinder 232 is fixedly provided with a baffle 235 which plays a role in stirring flow, the liquid is provided with a cyclone centrifugal effect through the baffle 235, a guide air pipe 236 which plays a role in guiding is fixedly arranged in a central through hole of the baffle 235, a quick connector 237 is arranged at the top pipeline of the guide air pipe 236, and the inner side wall of the adsorption inner cylinder 232 is provided with a groove which plays a role in blocking flow.
The dewatering assembly 25 comprises a dewatering cylinder 251, a dewatering cylinder 251 which plays a dewatering role is fixedly arranged at the bottom side of the left end of the preparation tank 1, a third reversing valve 252 is arranged at a water outlet pipeline at the bottom of the dewatering cylinder 251, a reversing effect is provided for washing wastewater through the third reversing valve 252, the bottom of the third reversing valve 252 is arranged at the bottom pipeline of the first reversing valve 22 through a connecting pipe, a fine pore filter cylinder 253 which plays a filtering role is rotatably arranged at the bottom of the inside of the dewatering cylinder 251 through a bracket, a water filtering cloth 254 which plays a filtering role is fixedly adhered to the inner side wall of the fine pore filter cylinder 253, a filtering blocking effect is provided through the fine Kong Lvtong and the water filtering cloth 254, a toothed ring 255 which plays a driving role is arranged at the outer side of a connecting plate at the top of the fine pore filter cylinder 253 through bolts, the outer side of the toothed ring 255 is meshed with the rear end of a driving gear 256, a center hole of the driving gear 256 is connected with a driving shaft of a servo motor 257, driving force is provided for the driving gear through the servo motor 257, the servo motor 257 is arranged inside a protection box at the front side of the dewatering cylinder 251 through bolts, the third reversing valve 252 and the servo motor 257 are electrically connected with a controller 6, and electric energy is provided for the third reversing valve 252 and the servo motor 257.
The detection assembly 28 comprises a connecting sleeve 281, a connecting sleeve 281 with a flow guiding function is arranged on the rear end pipeline of the return pipe 27, a fourth reversing valve 282 with a guiding function is arranged on the rear end pipeline of the connecting sleeve 281, a fifth reversing valve 284 with a guiding function is arranged on the top pipeline of the detection barrel 283, a magnet vibrator 285 with a detection function is arranged on the left end bolt of the detection barrel 283 through the fourth reversing valve 282 and the fifth reversing valve 284, a detector 286 is arranged on the rear end bolt of the detection barrel 283, a sample measuring electrode 287 is fixedly arranged on the upper side of the front end of the detector 286 through a wire, a reference electrode 288 is fixedly arranged on the lower side of the front end of the detector 286 through a wire, and the fourth reversing valve 282, the fifth reversing valve 284, the magnet vibrator 285, the detector 286, the sample measuring electrode 287 and the reference electrode 288 are all electrically connected with the controller 6, so that electric energy is provided for the fourth reversing valve 282, the fifth reversing valve 284, the vibrator 285, the detector 288, the sample measuring electrode 288 and the reference electrode 288.
The baffle 235 is spirally distributed on the inner wall of the inner adsorption cylinder 232, and the diameter of a central through hole of the baffle 235 and the air outlet pipe 236 provide a rotational flow effect for liquid in the inner adsorption cylinder 232 through the baffle 235.
The filter screen diameters of the fine-pore filter 253 and the water filter cloth 254 are 1 cm and 1 mm, respectively, and a filtering effect is provided for the preparation solution through the fine-pore filter 253 and the water filter cloth 254.
The front end of the dewatering cylinder 251 is provided with a connecting box body which plays a role in protecting the servo motor 257, and the connecting box body provides a protection effect for the servo motor 257.
The top of the fourth reversing valve 282 and the bottom of the fifth reversing valve 284 are respectively provided with a second outer connecting pipe 29, quick connectors are respectively arranged at the ends of the two groups of second outer connecting pipes 29, and liquid guiding effects are provided for the fourth reversing valve 282 and the fifth reversing valve 284 through the second outer connecting pipes 29.
The invention provides a preparation method of calcium fluoride powder for cores through improvement, which has the following working principle;
Firstly, when the equipment is used, the equipment is firstly placed in a working area, and then the device is connected with an external power supply, so that the power supply required by the work of the equipment can be provided;
Secondly, when preparation work is carried out, a worker adds quantitative distilled water into a reaction tank 8 in the preparation tank 1, then external hot water is led into the preparation tank 1 through a hot water conduit 9 and heated in the reaction tank 8, the distilled water can be kept at 60-80 ℃ through temperature control of the external hot water, then quantitative ammonium bifluoride raw materials are added into the reaction tank 8, the solid-to-liquid ratio of the ammonium bifluoride raw materials to the distilled water is 1:5, and then a transmission motor 5 is controlled by a controller 6 to work and drive a stirring paddle 7 to be stirred, so that the ammonium bifluoride raw materials and the distilled water are fully dissolved;
Thirdly, the calcium carbonate raw material is slowly and quantitatively introduced into the reaction tank 8 through the vibration of the discharging bin 3 and is dissolved through stirring, and the ratio of the calcium carbonate raw material to the mixed liquid is 1:7, keeping the temperature inside the reaction tank 8 between 60 and 80 ℃ under the action of the heat of the hot water conduit 9, fully reacting under the stirring action of the stirring paddle 7, guiding the mixed solution into the detection assembly 28 for detection under the driving action of the guiding-out pump 21 and the first reversing valve 22, guiding out the mixed liquid inside the reaction tank 8 through the guiding-out pump 21, and enabling the mixed liquid to flow into the adsorption inner cylinder 232 under the driving action of the first reversing valve 22;
Fourth, the leading-out pump 21 provides leading-out pressure for the liquid at this time, so that the mixed liquid with the reaction crystals forms a rotational flow state under the choked flow action of the baffle 235, and meanwhile, the external refrigerant is led into the heat exchange tube 233 through the external valve 234, so that the heat of the whole adsorption inner tube 232 is taken away, and the mixed liquid can be contacted with the inner wall of the adsorption inner tube 232 under the action of rotational flow centrifugation, so that the gas in the mixed liquid can be contacted with the adsorption inner tube 232 to separate from the liquid due to the condensation action of the liquid, so that liquid particles can be attached to the inner side of the adsorption inner tube 232, and the liquid particles are prevented from being taken away by the air flow through the groove strips on the inner side of the adsorption inner tube 232, thereby being beneficial to improving the separation of the gas generated by the reaction in the mixed liquid;
Fifthly, introducing the deaerated mixed liquid into the dehydration assembly 25 under the action of the second reversing valve 24, collecting the mixed liquid flowing in through the fine pore filter cylinder 253 and the water filtering cloth 254, controlling the servo motor 257 by the controller 6 to drive the transmission gear 256 to rotate and mesh with the toothed ring 255, driving the toothed ring 255 to rotate the fine pore filter cylinder 253 and the water filtering cloth 254, separating the redundant fluorine-containing wastewater from the calcium fluoride solid by the filtering effect of the fine pore filter cylinder 253 and the water filtering cloth 254 and the centrifugal force during rotation, guiding the redundant fluorine-containing wastewater out through the third reversing valve 252, and introducing external distilled water into the fine pore filter cylinder 253 to perform washing and washing actions by the guiding effect of the second reversing valve 24 and the second outer connecting pipe 29;
Sixth, at this time, the washing wastewater is led into the first reversing valve 22 due to the reversing effect of the third reversing valve 252, and flows into the detecting cylinder 283 through the reversing effects of the first reversing valve 22 and the fourth reversing valve 282, and the magnetite vibrator 285 is controlled to perform oscillation operation by the controller 6, the sample electrode 287 and the reference electrode 288 are subjected to oscillation waves to generate detection data and transmit the detection data to the detector 286, the detector 286 monitors the washing PH value through two sets of data, and the PH values of liquid and solid in the washing process are kept consistent, so that PH value data of calcium fluoride solid is obtained, and meanwhile, the parts such as the sample electrode 287 and the reference electrode 288 can be washed through the second external connecting pipe 29 to be led into external distilled water, so that the data influence among multiple detections is reduced, and the inside of the reaction tank 8 can be washed by using the washing wastewater which is gradually diluted; when the PH value data reaches the standard value, the repeated washing is stopped, and the calcium fluoride solid is taken out for drying and grinding.
The invention provides a preparation method of calcium fluoride powder for nuclear use, which is improved by arranging a preparation assembly 2 at the left end of a preparation tank 1, providing a multidirectional flow guiding effect for preparing solution through a guide pump 21 and a first reversing valve 22, intelligently controlling each preparation step through components such as a second reversing valve 24 and the like, being beneficial to improving the intelligent control effect on the preparation steps, arranging a gas filtering assembly 23 at the left end of the preparation tank 1, separating gas in liquid through the condensation effect of an adsorption inner cylinder 232 and a heat exchange tube 233, generating centrifugal force for preparing solution through the swirling effect of a baffle 235 to improve the gas-liquid separation effect, arranging a dehydration assembly 25 at the left end of the preparation tank 1, respectively driving a filter cylinder 253 and a toothed ring 255 to rotate at high speed through the filtering effect of the filter cylinder 253 and a water filtering cloth 254, and enabling a detection cylinder 283 to form a closed loop with the detection cartridge 283 and form a detection value of a detector through the flow guiding effect of a third reversing valve 284 and a fourth reversing valve 284 at the rear side of the preparation tank 1, and detecting the pH value of a reference electrode 288 under the detection value of a detector 285 and a reference electrode 286.
The basic principle and main characteristics of the invention and the advantages of the invention are shown and described above, standard parts used by the invention can be purchased from market, special-shaped parts can be customized according to the description of the specification and the drawings, the specific connection modes of the parts adopt conventional means such as mature bolt rivets and welding in the prior art, the machinery, the parts and the equipment adopt conventional models in the prior art, and the circuit connection adopts conventional connection modes in the prior art, so that the description is omitted.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (7)
1. The preparation equipment of the calcium fluoride powder for the nuclear comprises a preparation tank (1), wherein the preparation tank (1) is fixedly provided with a discharging bin (3) with a quantitative discharging function and a liquid injection port (4) with a liquid injection function at the top of the preparation tank (1);
The method is characterized in that: still including setting up at preparation subassembly (2) of preparation jar (1) left end, preparation subassembly (2) include:
the bottom through holes of the preparation tank (1) and the reaction tank (8) are connected with a water inlet pipeline at the top of the export pump (21) through connecting pipes;
The first reversing valve (22) is arranged at the rear end water outlet pipeline of the guide pump (21), and the first reversing valve (22) has a guiding function;
The left end of the first reversing valve (22) is fixedly provided with the air filtering component (23) through a connecting pipe;
The second reversing valve (24) is arranged at the bottom pipeline of the air filtering assembly (23), and the second reversing valve (24) has a control function;
the bottom of the second reversing valve (24) is provided with a dehydration assembly (25) which plays a role in dehydration;
the first external connection pipe (26) is arranged at the water inlet pipeline at the rear end of the second reversing valve (24);
the return pipe (27) is arranged at the rear end water outlet pipeline of the first reversing valve (22), and the return pipe (27) has a return function;
the rear end of the return pipe (27) is provided with a detection component (28) which plays a role in detection;
the top of the detection component (28) is provided with a second outer connecting pipe (29);
The connection parts at the outer sides of the first outer connecting pipe (26) and the second outer connecting pipe (29) are respectively provided with a quick connector, and the leading-out pump (21), the first reversing valve (22) and the second reversing valve (24) are electrically connected with the controller (6);
The air filter assembly (23) comprises:
a temperature control outer cylinder (231), wherein the top side of the left end of the preparation tank (1) is fixedly provided with the temperature control outer cylinder (231);
An adsorption inner cylinder (232), wherein the inner side wall of the temperature control outer cylinder (231) is fixedly provided with the adsorption inner cylinder (232) which plays a role in separation and adsorption through bolts;
a heat exchange tube (233), wherein the heat exchange tube (233) playing a role in heat exchange is adhered and fixed on the outer side wall of the adsorption inner cylinder (232);
the water inlets and the water outlets on the upper side and the lower side of the heat exchange tube (233) are connected with the external valve (234) through pipelines;
The baffle plate (235) is fixedly welded on the inner side wall of the adsorption inner cylinder (232), and the baffle plate (235) plays a role in stirring flow;
the air guiding pipe (236) is welded and fixed at the central through hole of the baffle plate (235), and the air guiding pipe (236) has a guiding function;
The quick connector (237) is arranged on the top pipeline of the air outlet pipe (236);
Wherein, the inner side wall of the adsorption inner cylinder (232) is provided with a groove which plays a role of choking flow;
The dewatering assembly (25) comprises:
a dewatering cylinder (251), wherein the bottom side of the left end of the preparation tank (1) is fixedly provided with the dewatering cylinder (251) which plays a role in dewatering;
the third reversing valve (252) is arranged on a water outlet pipeline at the bottom of the dehydration cylinder (251);
the bottom of the third reversing valve (252) is arranged with a bottom pipeline of the first reversing valve (22) through a connecting pipe;
The inner bottom of the dehydration cylinder (251) is rotatably provided with the fine pore filter cylinder (253) which plays a role in filtration through a bracket;
A water filtering cloth (254), wherein the water filtering cloth (254) playing a role in filtering is adhered and fixed on the inner side wall of the fine pore filter cylinder (253);
the gear ring (255) is arranged on the outer side of the connecting plate at the top of the fine-hole filter cylinder (253) through bolts, and the gear ring (255) has a transmission function;
the outer side of the toothed ring (255) is meshed with the rear end of the transmission gear (256);
The servo motor (257), the centre hole of the transmission gear (256) is connected with a transmission shaft key of the servo motor (257);
the servo motor (257) is mounted in the front side protection box of the dewatering cylinder (251) through bolts, and the third reversing valve (252) and the servo motor (257) are electrically connected with the controller (6);
the detection assembly (28) includes:
A connecting sleeve (281), wherein a connecting sleeve (281) with a diversion function is arranged at the rear end pipeline of the return pipe (27);
the rear end pipeline of the connecting sleeve (281) is provided with a fourth reversing valve (282) with a guiding function;
The fourth reversing valve (282) is arranged at the bottom of the detection cylinder (283) in a pipeline manner;
A fifth reversing valve (284), wherein a fifth reversing valve (284) with a guiding function is arranged on the top pipeline of the detection cylinder (283);
A magnet vibrator (285), wherein the magnet vibrator (285) playing a role in detection is mounted on the bolt at the left end of the detection cylinder (283);
A detector (286), the detector (286) is mounted on the rear end bolt of the detection barrel (283);
A sample electrode (287), wherein the upper side of the front end of the detector (286) is fixedly provided with the sample electrode (287) through a lead;
The reference electrode (288) is fixedly arranged on the lower side of the front end of the detector (286) through a wire;
The fourth reversing valve (282), the fifth reversing valve (284), the magnet vibrator (285), the detector (286), the sample measuring electrode (287) and the reference electrode (288) are all electrically connected with the controller (6).
2. The apparatus for producing calcium fluoride powder for nuclear use according to claim 1, wherein: the utility model discloses a preparation jar, including preparation jar (1), drive motor (5) are installed to side bolt in preparation jar (1) top and bolt installs controller (6) at preparation jar (1) front side, drive motor (5) bottom transmission shaft fixed mounting has stirring rake (7) that play the stirring effect, stirring rake (7) rotate and set up inside retort (8), preparation jar (1) front end bottom side is equipped with hot water pipe (9).
3. The apparatus for producing calcium fluoride powder for nuclear use according to claim 2, wherein: the baffle plates (235) are spirally distributed on the inner wall of the adsorption inner cylinder (232), and the diameter of a central through hole of each baffle plate (235) and the diameter of a gas guiding-out pipe (236) are equal.
4. A production apparatus of calcium fluoride powder for nuclear use according to claim 3, wherein: the filter screen diameters of the fine pore filter cylinder (253) and the water filtering cloth (254) are 1 cm and 1 mm respectively.
5. The apparatus for producing calcium fluoride powder for core according to claim 4, wherein: the front end of the dehydration cylinder (251) is provided with a connecting box body which plays a role in protecting the servo motor (257).
6. The apparatus for producing calcium fluoride powder for core according to claim 5, wherein: the top of the fourth reversing valve (282) and the bottom of the fifth reversing valve (284) are respectively provided with a second outer connecting pipe (29), and quick connectors are respectively arranged at the ends of the two groups of second outer connecting pipes (29).
7. A production method using the production apparatus of calcium fluoride powder for nuclear use according to any one of claims 1 to 6, characterized in that: the method comprises the following steps:
step one: quantitatively adding distilled water and ammonium bifluoride raw materials: adding quantitative distilled water into a reaction tank (8) in a preparation tank (1), introducing external hot water into the preparation tank (1) through a hot water conduit (9), heating distilled water in the reaction tank (8), controlling the temperature of the external hot water to enable the distilled water to be kept at 60-80 ℃, adding quantitative ammonium bifluoride raw material into the reaction tank (8), proportioning the ammonium bifluoride raw material and distilled water at a solid-to-liquid ratio of 1:5, and controlling a transmission motor (5) to work through a controller (6) and driving a stirring paddle (7) to stir, so that the ammonium bifluoride raw material and distilled water are fully dissolved;
Step two: quantitative and slow addition of calcium carbonate raw material: then the calcium carbonate raw material is slowly and quantitatively introduced into the reaction tank (8) through the vibration of the discharging bin (3), and is dissolved through stirring, wherein the ratio of the calcium carbonate raw material to the mixed liquid is 1:7, keeping the temperature inside the reaction tank (8) between 60 and 80 ℃ under the action of the heat of the hot water conduit (9), fully reacting under the stirring action of the stirring paddle (7), and leading the mixed solution into the detection assembly (28) for detection under the driving action of the leading-out pump (21) and the first reversing valve (22);
Step three: and (3) guiding out filtered gas: then, the mixed liquid in the reaction tank (8) is guided out through the guiding-out pump (21) and flows into the adsorption inner cylinder (232) under the driving action of the first reversing valve (22), guiding-out pressure is provided for the liquid through the guiding-out pump (21), so that the mixed liquid with the reaction crystals forms a rotational flow state under the choked flow action of the baffle plate (235), and meanwhile, the external refrigerant is guided into the heat exchange tube (233) through the external valve (234), so that the heat of the whole adsorption inner cylinder (232) is taken away, the mixed liquid can be contacted with the inner wall of the adsorption inner cylinder (232) under the action of rotational flow centrifugation, so that the gas in the mixed liquid can be contacted with the adsorption inner cylinder (232) to separate from the liquid under the condensation action of the liquid, and liquid particles can be attached to the inner side of the adsorption inner cylinder (232), and the mixed liquid is prevented from being taken away by air flow through the groove strips on the inner side of the adsorption inner cylinder (232), and the separation of the gas generated by the reaction in the mixed liquid is facilitated;
Step four: and (3) centrifugal dehydration: then introducing the deaerated mixed liquid into a dehydration assembly (25) under the action of a second reversing valve (24), collecting the inflow mixed liquid through a fine-hole filter cylinder (253) and a water filtering cloth (254), controlling a servo motor (257) to drive a transmission gear (256) to rotate and enable the transmission gear to be meshed with a toothed ring (255) through a controller (6), enabling the toothed ring (255) to drive the fine-hole filter cylinder (253) and the water filtering cloth (254) to rotate, separating redundant fluorine-containing wastewater from calcium fluoride solids through the filtering effect of the fine-hole filter cylinder (253) and the water filtering cloth (254) and centrifugal force during rotation, and guiding the redundant fluorine-containing wastewater out through a third reversing valve (252);
step five: repeat the washing: the external distilled water is led into the fine pore filter cylinder (253) through the flow guiding effect of the second reversing valve (24) and the second external connecting pipe (29) to carry out washing and washing actions on the calcium fluoride solid;
Step six: and (3) pH value detection: at the moment, the washing wastewater is guided into the first reversing valve (22) due to the reversing effect of the third reversing valve (252), flows into the detection cylinder (283) through the reversing effects of the first reversing valve (22) and the fourth reversing valve (282), and is controlled by the controller (6) to perform oscillation operation on the magnetite vibrator (285), the detection data are generated by the oscillation waves of the sample measuring electrode (287) and the reference electrode (288) and are transmitted to the detector (286), the detector (286) monitors the washing pH value through two groups of data, and the pH value of liquid and solid in the washing process is kept consistent, so that the pH value data of calcium fluoride solid are also obtained;
step seven: grinding and pulverizing: when the pH value data reaches the standard value, the repeated washing is stopped, and the calcium fluoride solid is taken out for drying and grinding.
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Denomination of invention: Preparation method of nuclear calcium fluoride powder Granted publication date: 20240416 Pledgee: Bank of China Limited by Share Ltd. Shanghai Jingan branch Pledgor: Shanghai Taiyang Technology Co.,Ltd. Registration number: Y2024310000636 |